Process for obtaining valuable distillates from carbonaceous materials



Dec. 19, 1933. R. P. RUSSELL 1,940,648

PROCESS FOR OBTAINING VALUABLE DISTILLATES FROM CARBONACEOUS MATERIALSFiled Jan. 22, 1929 $7M 0. M Svwemtoz J Patented Dec. 19, 1933 PATENTOFFICE PROCESS FOR OBTAINING VALUABLE DISTILLATES F R O M CARBONACEOUSMATERIALS Robert P. Russell, Baton Rouge, La., assignor to Standard-I.G. Company Application January 22, 1929. Serial No. 334,148

' Claims.

The present invention comprises an improved process for obtainingvaluable low boiling oils from carbonaceous materials such as petroleum,tars and the like and also from solid carbona- 5 ceous materialsespecially those, which like coal, contain solid foreign matter. Myprocess will be fully understood from the following description and thedrawing.

The drawing is a semi-diagrammatic view in sectionalzelevation of anapparatus constructed according to my invention and indicates the fiowof materials.

Referring to the drawing, reference numeral 1 denotes a pipe coilarranged in a suitablefurnace setting 2 and adapted to heat a stream ofhydrocarbon oil or the like to an elevated temperature. The coildischarges into a reaction chamber 3 which is constructed to withstandhigh internal pressure and high temperature,

as well as the corrosive eifects of the reactants.

The contents of the drum is kept in thorough agitation by means of astirrer 4 or the like and the temperature of the drum is maintained atthe desired level in any suitable manner, for example, by the use ofinternal electrical heaters. but I prefer to continuously withdraw apartof the oil by pipe 5 and circulate the same by means of a suitable pump6 back to drum 3 by way of coil 1. Hydrogen or a gas rich in freehydrogen is withdrawn from a suitable source (not shown) by pipe 7,compressed by a compressor 8 and then conducted by pipe 9 to a feedmanifold 10 from which a part may be forced into the inlet of coil 1 byline 11 and the remainder introduced directly into drum 3 by line 12.The drum is preferably protected against excessive loss of heat as byinsulation 13.

Vapor from drum 3 is conducted by vapor line 14 to a heat exchanger 15,then to a condenser 16 and gas separator 17. Distillate is conducted tostorage (not shown) by pipe 17' while gas is recompressed by boosterpump 18 and returned to hydrogen manifold 10 by pipe 18'. The gas may bepurified before return to the manifold,

for example, by washing with an aqueous soda solution to remove hydrogensulphide and then with oil to remove gaseous hydrocarbons.

A part of the oily mass undergoing treatr n ent is withdrawn from drum3, preferably in a continuous stream, by a line 19 which is fitted witha pressure reduction valve 20 and is discharged into a chamber 21.Chamber 21 may be of any suitable form, with or without ba flles 22, butwith a lower chamber 23 which is furnished with a double bell closure23' or. other suitable means for discharging solid or semi-solidmaterials intermittently. A vapor pipe 24 conducts vaporized oil tocondenser 25 and discharges it into 'a separator 26 from which gas isremoved, by vacuum pump 28. Condensate is withdrawn from separator 26 bypump 29 and is returned to drum 4 as will be described below. A currentof inert gas may be passed into drum 21 by pipe 21a in order to assistin the vaporization of the liquid after reduction of pressure.

Fresh oil is drawn from storage (not shown) by pump 31 and a part may bediverted through a pulverizer 32 in which coal or other solidcarbonaceous material is reduced to a finely divided state andthoroughly incorporated with the oil. Condensate from drum 26 is forcedby pump 29 through a line 30 into a branch pipe so that it may be passedthrough pulverizer 32 or may be added to the mixture of oil and coal asshown in the drawing. In any case the mixture is then forced throughheat exchanger 15 to coil 1 by line 34.

In the operation of my process, crude oils, tar and the like may be usedas the base and carbonaceous material which contains ash or otherforeign solid impurities is suspended in the oily liquid. Such materialis subjected to the action of a gas rich in free hydrogen under a highpressure, for example, above about 25 atmospheres and preferably at 100or 200 atmospheres or higher. The body of material which is in asemiliquid, at least pumpable form, is maintained at a temperaturewithin the approximate range of 750 to 850 degrees Fahrenheit. Hydrogenis continuously forced into the body of oily material and vapor whichcomprises distillate and gas is continuously removed during thehydrogenation.

Part of the oily mixture is withdrawn from drum 3 and discharged into achamber 21 which is. maintained at a pressure considerably lower thandrum 3. By this means, a large part of the oil withdrawn is vaporizedand separated from solid matter, such as ash, free carbon, unvaporlzableasphaltic residue, and the like. The distillation is preferably doneunder vacuum and the 100 solid matter may be obtained in substantiallydry form, at least, freed from the majority of the oil which iscondensed and preferably returned to the body of material undergoinghydrogenation in drum 3.

When a relatively large proportion of coal is used with the oil, thereaction is strongly exothermic and furnishes sufflcient' heat tomaintain temperature in the'drum without internal heating or the like,and coil 1 may be used merely 110- as a preheating coil for the freshsuspension of carbonaceous material in oil. It will be understood that,if desired, fresh oil need not be continuously supplied; but after thecycle has been established, heavy oil may be produced in sufficientquantity to furnish the suspension medium for the entire quantity ofcoal or other carbonaceous material heated.

My invention is not to be limited by any theory of the process, nor bymerely an illustrative example, but only by the following claims-inwhich I wish to claim all novelty inherent in the invention. a

I claim:

1. An improved process for production of low boiling liquid hydrocarbonsfrom solid carbonaceous materials comprising, forming a suspension offinely ground carbonaceous material in heavy oil, maintaining a body ofthe suspension at a decomposition temperature and under high pressure,continuously forcing a hot mixture of the suspension and a gas rich infree hydrogen into the body, continuously withdrawing vapor therefrom,condensing low boiling liquid hydrocarbon from the vapor, separatelywithdrawing a part of the suspension from the body, reducing pressure onthe part thus withdrawn whereby substantially all of the oil isvaporized, condensing the vapor and returning a part of the condensateto the body of the material undergoing treatment.

2. Process according to claim 1 in which the suspension of solidmaterial in oil is maintained at a temperature of approximately 750-850degrees Fahrenheit and under pressure in excess of 25 atmospheres.

3. In a process for the liquefaction of coal the steps of maintaining abody of finely divided coal suspended in heavy oil at high temperatureand 7 under high pressure of hydrogen, continuously removing the vaporsevolved therefrom, separately withdrawing a part of the suspensioncontaining ash, reducing pressure on the part withdrawn whereby theliquid is substantially completely vaporized, separately condensing thisvapor and returning the condensate to the, body of coal and oil.

4. An improved process for producing valuable liquid hydrocarbons fromsolid carbonaceous material which comprises reducing such material to afinely divide'd state, suspending the same in heavy hydrocarbon oil,maintaining a body of such suspension at an elevated temperature andunder high pressure in contact with a gas rich in free hydrogen,continuously removing vapors from the body of suspension, separatelywithdrawing a part of the suspension from the body, reducing pressure onthe part withdrawn whereby a substantial portion of the hydrocarbonliquid is vaporized, passing a current of inert gas through the residueafter reduction of pressure, and separately condensing the vapor evolvedby the reduction of pressure.

5. An improved process for producing liquid hydrocarbons from solidcarbonaceous material 100 which comprises reducing such material to afinely divided state, suspending the same in heavy hydrocarbon oil,subjecting a body of such suspension to the action of a gas rich in freehydrogen at an elevated temperature and under 105 high pressure,continuously removing vapors from the body of suspension, separatelywithdrawing a portion of the suspension from the mass undergoinghydrogenation, reducing pressure on the portion withdrawn to asub-atmospheric pres- 110 sure whereby a substantial portion of thehydrocarbon liquid is vaporized, and separately eondensing the vapor.

ROBERT P. RUSSELL.

